反应详情

温度

-15 °C

Phosphoryl chloride (0.03 ml) was added dropwise to a stirred mixture of N-(3-amino-4-chlorophenyl)-4-cyanobenzamide (0.08 g), 4-(2-ethoxyethoxy)benzoic acid (J. Org. Chem., 1973, 38, 3160; 0.062 g) and pyridine (4 ml) which had been cooled to −15° C. The reaction mixture was stirred at −15° C. for 3 hours and then allowed to warm to ambient temperature. The mixture was stirred for 48 hours. The reaction mixture was diluted with water and stirred overnight. The precipitate was isolated, washed with diethyl ether and dried under vacuum at 55° C. to give the title compound (0.024 g); NMR Spectrum: (DMSOd6) 1.15 (t, 3H), 3.49 (m, 2H), 3.73 (m, 2H), 4.19 (m, 2H), 9.86 (s, 1H), 10.62 (s, 1H); Mass Spectrum: M−H− 462.

1. temperatureto warm to ambient temperature
2. stirringThe mixture was stirred for 48 hours
3. stirringstirred overnight
4. customThe precipitate was isolated
5. washwashed with diethyl ether
6. customdried under vacuum at 55° C.